CN118103688A - Contact and method for evaluating micro-wear characteristics of single crystal diamond using same - Google Patents
Contact and method for evaluating micro-wear characteristics of single crystal diamond using same Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 185
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 185
- 239000013078 crystal Substances 0.000 title claims description 115
- 238000000034 method Methods 0.000 title description 19
- 239000002245 particle Substances 0.000 claims abstract description 35
- 238000011156 evaluation Methods 0.000 claims description 31
- 238000003825 pressing Methods 0.000 claims description 13
- 238000012360 testing method Methods 0.000 description 53
- 238000005299 abrasion Methods 0.000 description 43
- 239000012535 impurity Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000005259 measurement Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910001018 Cast iron Inorganic materials 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/56—Investigating resistance to wear or abrasion
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- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Measuring Leads Or Probes (AREA)
Abstract
A contact made of polycrystalline diamond composed of a plurality of diamond particles, the contact being formed in a ring shape so that a rotation axis passes through the center, the contact comprising: a first portion having a constant thickness in a radial direction and including an inner end portion; and a second portion having a radially reduced thickness and comprising an outer end, the second portion having: a first face continuous with an upper surface of the first portion; a second surface continuous with a lower surface of the first portion; and a connection surface connecting the first surface and the second surface and including the outer end portion, wherein an angle θ formed by a first line segment representing the first surface and a second line segment representing the second surface in a cross section along the rotation axis is 100 ° or more and 150 ° or less, a length between a first boundary portion that is a boundary between the first surface and the connection surface and a second boundary portion that is a boundary between the second surface and the connection surface is 1 μm or more and 10 μm or less, a length from the rotation axis to the outer end portion is 0.5mm or more and 5mm or less, and an average grain diameter of the plurality of diamond grains is 10nm or more and 300nm or less.
Description
Technical Field
The present disclosure relates to a contact and a method for evaluating micro wear characteristics of single crystal diamond using the same. The present application claims priority based on japanese patent application No. 2021-183404, 11/10 of 2021, and the entire contents of the description of the japanese patent application are incorporated herein by reference.
Background
In the industrial single crystal diamond, the distribution of nitrogen impurities and crystal defects varies depending on the crystal, and even if the crystal is the same, the wear characteristics vary depending on the region when observed in a minute region.
Therefore, in particular, when single crystal diamond is used as a tool material for precision machining, it is important to sufficiently grasp the difference in wear characteristics of each minute region in the same crystal in advance.
Methods of using a cast iron wheel or a metal bond diamond grinding wheel having a small diameter and a V-shaped cutting edge for evaluating wear characteristics in a micro region of single crystal diamond are known (non-patent document 1 and non-patent document 2).
Prior art literature
Non-patent literature
Non-patent literature 1：Eileen M.Wilks&J.Wilks.(1959)."The Resistance of Diamond to Abrasion".Philosophical.Magazine,4：38,158-170.
Non-patent literature 2：E M Wilks and J Wilks.(1972)."The resistance of diamond to abrasion".Journal of Physics D：Applied Physics,5,1902-1919.
Disclosure of Invention
The contact of the present disclosure is an annular contact made of polycrystalline diamond made of a plurality of diamond particles, wherein,
The contact is configured such that the rotation shaft passes through the center,
The contact is provided with:
a first portion having a constant thickness in a radial direction and including an inner end portion; and
A second portion having a radially reduced thickness and comprising an outer end portion,
The second portion has:
A first face continuous with an upper surface of the first portion; a second surface continuous with a lower surface of the first portion; and a connecting surface connecting the first surface with the second surface and including the outer end portion,
In a section along the axis of rotation,
An angle θ between a first line segment representing the first surface and a second line segment representing the second surface is 100 DEG or more and 150 DEG or less,
A length between a first boundary portion which is a boundary between the first surface and the connection surface and a second boundary portion which is a boundary between the second surface and the connection surface is 1 μm or more and 10 μm or less,
The length from the rotation shaft to the outer end is 0.5mm or more and 5mm or less,
The plurality of diamond particles have an average particle diameter of 10nm to 300 nm.
The evaluation method of the present disclosure is an evaluation method of wear characteristics in a micro region of single crystal diamond,
The evaluation method includes:
a first step of pressing the single crystal diamond toward the outer end portion while rotating the contact, thereby forming a wear mark on the single crystal diamond; and
And a second step in which wear characteristics in a micro region of the single crystal diamond are evaluated based on the length of the wear trace.
Drawings
Fig. 1 is a photograph substitute drawing showing an appearance of an example of a contact according to an embodiment of the present disclosure.
Fig. 2 is a top view of one example of a contact according to one embodiment of the present disclosure.
Fig. 3 is a cross-sectional view taken along line XI-XI of the contact shown in fig. 2.
Fig. 4 is an enlarged view of a second portion of the contact shown in fig. 3.
Fig. 5 is a cross-sectional view of a second portion according to other embodiments of the present disclosure.
Fig. 6 is an overview of a wear test device used for a method of evaluating wear characteristics in a micro-region of a single crystal diamond according to an embodiment of the present disclosure.
FIG. 7 is a diagram showing the < 100 > direction and the < 110 > direction of the (001) plane of single crystal diamond.
Fig. 8 is a photograph substitute graph showing the abrasion trace formed in example 1.
Fig. 9 is a photograph substitute graph showing the abrasion trace formed in example 2.
Fig. 10 is a graph showing the relationship between the test numbers and the wear mark lengths in example 1 and example 2.
FIG. 11 is a photograph substitute drawing showing an ultraviolet excited fluorescent image of the specimen A.
Fig. 12 is a graph showing the relationship between the test number and the wear mark length in the test body a.
FIG. 13 is a photograph substitute drawing showing an ultraviolet excited fluorescent image of the specimen B.
Fig. 14 is a graph showing the relationship between the test number and the wear mark length in the test body B.
Detailed Description
[ Problem to be solved by the present disclosure ]
Since the cast iron wheel described in non-patent document 1 is softer than single crystal diamond, the tip is easily deformed in the wear test and no wear mark is left in the wear direction. In addition, the diamond powder of the abrasive material flies up and the sharpness is immediately passivated. Therefore, it is difficult to quantitatively and appropriately evaluate the wear characteristics in the micro-regions of the single crystal diamond.
When the metal bond diamond grinding wheel described in patent document 2 is used for a single crystal diamond material, diamond abrasive grains are likely to fall off, and the shape of the cutting edge is likely to be deformed. On this basis, the grinding performance of the tip is unstable due to the deviation of the grain size and strength of the diamond abrasive grains. Therefore, it is difficult to quantitatively and appropriately evaluate the wear characteristics in the micro-regions of the single crystal diamond.
Accordingly, an object of the present disclosure is to provide a contact for use in a method of evaluating wear characteristics in a micro-region of a single crystal diamond and a method of evaluating wear characteristics in a micro-region of a single crystal diamond using the contact.
[ Effect of the present disclosure ]
According to the present disclosure, a contact for wear characteristics in a micro region of single crystal diamond can be provided. The contact can be used to evaluate the wear characteristics in the micro-region of the single crystal diamond.
[ Description of embodiments of the present disclosure ]
First, embodiments of the present disclosure are listed and described.
(1) The contact of the present disclosure is an annular contact made of polycrystalline diamond made of a plurality of diamond particles, wherein,
The contact is configured such that the rotation shaft passes through the center,
The contact is provided with:
a first portion having a constant thickness in a radial direction and including an inner end portion; and
A second portion having a radially reduced thickness and comprising an outer end portion,
The second portion has:
A first face continuous with an upper surface of the first portion; a second surface continuous with a lower surface of the first portion; and a connecting surface connecting the first surface with the second surface and including the outer end portion,
In a section along the axis of rotation,
An angle θ between a first line segment representing the first surface and a second line segment representing the second surface is 100 DEG or more and 150 DEG or less,
A length between a first boundary portion which is a boundary between the first surface and the connection surface and a second boundary portion which is a boundary between the second surface and the connection surface is 1 μm or more and 10 μm or less,
The length from the rotation shaft to the outer end is 0.5mm or more and 5mm or less,
The plurality of diamond particles have an average particle diameter of 10nm to 300 nm.
According to the present disclosure, the wear characteristics in the micro-regions of the single crystal diamond can be evaluated (in this specification, the wear characteristics in the micro-regions are also described as "micro-wear characteristics").
(2) The knoop hardness of the polycrystalline diamond may be 120GPa or more. This improves the accuracy of the evaluation of the micro wear characteristics.
(3) The intersection of the connection surface and the cross section including the rotation axis may be a straight line. Thus, the evaluation result of the micro wear characteristic is stable.
(4) The length from the rotation axis to the outer end portion may be longer than the length from the rotation axis to the first boundary portion and longer than the length from the rotation axis to the second boundary portion. Thus, the evaluation result of the micro wear characteristic is stable.
(5) The evaluation method of the present disclosure is an evaluation method of wear characteristics in a micro region of single crystal diamond, wherein,
The evaluation method includes:
A first step of pressing the single crystal diamond toward the outer end portion while rotating the contact, thereby forming a wear mark on the single crystal diamond; and
And a second step in which wear characteristics in a micro region of the single crystal diamond are evaluated based on the length of the wear trace.
According to the present disclosure, wear characteristics in a micro region of single crystal diamond can be evaluated.
(6) The single crystal diamond has a planar surface and,
The first step may also comprise:
A step 1-1 in which the single crystal diamond is arranged such that the plane faces the contact and is parallel to the rotation axis in the step 1-1; and
And 1-2 steps of pressing the single crystal diamond toward the outer end portion by applying a load in a normal direction of the third plane to the single crystal diamond in the 1-2 steps.
This improves the accuracy of the evaluation of the micro wear characteristics.
(7) The third plane may be a (001) plane, and the abrasion trace may be parallel to a < 100 > direction of the (001) plane. This improves the accuracy of the evaluation of the micro wear characteristics.
Detailed description of embodiments of the disclosure
The contact of the present disclosure and a method for evaluating the micro wear characteristics of single crystal diamond using the contact are described below with reference to the drawings. In the drawings of the present disclosure, like reference numerals designate like or corresponding parts. The dimensional relationships such as length, width, thickness, and depth are appropriately changed for the sake of clarity and simplicity of the drawings, and do not necessarily represent actual dimensional relationships. For convenience of explanation, fig. 3, 4, and 5 are compressed in the longitudinal direction.
In the present specification, the expression "a to B" means the upper limit and the lower limit of the range (i.e., a to B below), and a is the same as B in the case where a is not described and only B is described.
Embodiment 1: contact piece
A contact according to an embodiment of the present disclosure (hereinafter, also referred to as "the present embodiment") will be described with reference to fig. 1 to 5. The contact 1 of the present embodiment is a ring-shaped contact 1 made of polycrystalline diamond composed of a plurality of diamond particles,
The contact 1 is configured such that a rotation axis R passes through the center,
The contact 1 includes:
a first portion 2 having a constant thickness in the radial direction and comprising an inner end; and
The second portion 3, having a radially reduced thickness and comprising an outer end 3A,
The second part 3 has:
A first face 31 continuous with the upper surface of the first portion 2; a second face 32 continuous with the lower surface of the first portion 2; and a connecting surface 33 connecting the first surface 31 and the second surface 32 and including an outer end portion 3A,
In a section along the axis of rotation R,
The angle theta between the first line segment representing the first surface 31 and the second line segment representing the second surface 32 is 100 DEG or more and 150 DEG or less,
The length between the first boundary portion 31A, which is the boundary between the first surface 31 and the connection surface 33, and the second boundary portion 32A, which is the boundary between the second surface 32 and the connection surface 33, is 1 μm or more and 10 μm or less,
The length from the rotation axis R to the outer end 3A is 0.5mm or more and 5mm or less,
The plurality of diamond particles have an average particle diameter of 10nm to 300 nm.
The contact according to the present embodiment is made of polycrystalline diamond composed of a plurality of diamond grains. Here, the polycrystalline diamond composed of a plurality of diamond grains means polycrystalline diamond in which diamond grains are directly bonded to each other. Polycrystalline diamond does not contain a binder phase (binder) formed of one or both of a sintering aid and a binder that are generally used for diamond sintered bodies, and is a polycrystalline body composed of a single phase of diamond.
The polycrystalline diamond may contain unavoidable impurities in addition to the diamond component as long as the effect of the present disclosure is exhibited. Examples of the unavoidable impurities include hydrogen (H), oxygen (O), nitrogen (N), sodium (Na), magnesium (Mg), aluminum (Al), silicon (Si), phosphorus (P), sulfur (S), chlorine (Cl), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), molybdenum (Mo), and the like.
The diamond component content of the polycrystalline diamond is preferably 99% by volume or more.
The polycrystalline diamond is composed of a diamond component and unavoidable impurities, and the diamond component content of the polycrystalline diamond is preferably 99% by volume or more. The polycrystalline diamond contains 99% by volume or more of diamond components, and can be confirmed by an X-ray diffraction method. The absence of the binder phase in the polycrystalline diamond can be confirmed by observing the surface of the polycrystalline diamond with an optical microscope and an electron microscope.
The average particle diameter of the plurality of diamond particles constituting the polycrystalline diamond (hereinafter, also referred to as "average particle diameter of diamond particles") is 10nm to 300 nm. That is, the polycrystalline diamond is a nano polycrystalline diamond (NPD: nano Polycrystalline Diamond) in which fine diamond particles of several tens nm are firmly bonded. The hardness of polycrystalline diamond has no azimuth dependence, and the polycrystalline diamond has higher hardness and strength than single crystal diamond.
The lower limit of the average particle diameter of the diamond particles is 10nm or more, or 20nm or more, or 30nm or more from the viewpoint of obtaining mechanical strength peculiar to diamond. The upper limit of the average particle diameter of the diamond particles is 300nm or less, 200nm or less, or 100nm or less, from the viewpoint that the polycrystalline diamond 75 can exhibit the hardness and wear resistance of the same property in all directions. The average particle diameter of the diamond particles is 10nm to 300nm, or 20nm to 200nm, or 30nm to 100 nm.
The average particle diameter of the diamond particles was determined by a cutting method using a Scanning Electron Microscope (SEM). Specifically, first, a scanning electron microscope is used to observe polycrystalline diamond at a magnification of 1000 to 100000 times, and an SEM image is obtained.
Next, a circle is drawn in the SEM image, and eight straight lines (such that the intersecting angles between the straight lines are almost equal) are radially drawn from the center of the circle to the outer periphery of the circle. In this case, the observation magnification and the diameter of the circle are set so that the number of diamond particles (crystal particles) crossing the straight line is about 10 to 50.
Next, for each of the straight lines, the number of crystal grain boundaries crossing the diamond grains was counted, the length of the straight line was divided by the number of the straight lines crossing the straight lines, and the average slice length was obtained, and the value obtained by multiplying the average slice length by 1.128 was the average grain diameter. The above measurement was performed on three SEM images, and the average particle diameter was determined for each of the three SEM images. The average particle diameter of the diamond particles in the present specification is an average value of the average particle diameters of three SEM images.
Note that, the following was confirmed: if the measurement is performed in the same sample, there is little variation in the measurement result even if the measurement is performed a plurality of times by changing the selected position of the measurement field of view, and the measurement field of view does not become random even if the measurement field of view is arbitrarily set.
When evaluating wear characteristics in a micro region of single crystal diamond 75 using contact 1, outer end 3A of contact 1 is brought into contact with single crystal diamond 75 while rotating contact 1 about rotation axis R, thereby forming a wear trace on single crystal diamond 75. Thus, the polycrystalline diamond constituting the contact according to the present embodiment may have a hardness equal to or greater than that of the single crystal diamond 75.
The hardness of single crystal diamond 75 varies from 70 to 120GPa depending on the face orientation. Accordingly, the Knoop hardness of the polycrystalline diamond may be 120GPa or more, 125GPa or more, or 130GPa or more. The upper limit of the knoop hardness of the polycrystalline diamond is not particularly limited, and may be 160GPa or less from the viewpoint of production. The knoop hardness of the polycrystalline diamond may be 120GPa to 160GPa, 125GPa to 155GPa, or 130GPa to 150 GPa.
In the present specification, the knoop hardness of polycrystalline diamond is measured by JIS Z2251: 2009. Specifically, a diamond-shaped knoop indenter was pressed against the surface of the polycrystalline diamond to generate an indentation with a test force of 4.9N for 10 seconds. The test temperature was set at 23 ℃ + -5 ℃. After the test force was released, the longer diagonal line length a (μm) of the indentation remaining on the surface of the polycrystalline diamond was measured, and the knoop Hardness (HK) was calculated by the following formula (1).
Hk=14229×f/a 2 (1)
As shown in fig. 1 to 3, the contact 1 includes: the first portion 2, and the second portion 3 continuous with the first portion 2 and surrounding the outer periphery of the first portion 2, the length of the second portion 3 in the direction of the rotation axis R decreases toward the outer end portion 3A in a section including the rotation axis R. Here, as shown in fig. 3, the length of the second portion 3 in the rotation axis R direction decreasing toward the outer end 3A means a relationship of L1 > L2 > L3 in which the length of the second portion 3 in the rotation axis R direction is L1, L2, and L3 in order from the rotation axis. As shown in fig. 2, the contact 1 has a circular diameter in a plan view. The maximum length of the contact 1in the direction of the rotation axis R is not particularly limited, and may be, for example, 0.2mm or more and 2mm or less.
The length R1 of the contact 1 in the direction perpendicular to the rotation axis R between the rotation axis R and the outer end 3A is 0.5mm or more and 5mm or less. Thus, the contact 1 is easy to handle, and a minute trace of wear can be formed on the single crystal diamond 75.
The lower limit of the length r1 is 0.5mm or more, or 1mm or more, or 1.5mm or more, from the viewpoint of ease of handling the contact 1. The upper limit of the length r1 is 5mm or less, or 3mm or less, or 2mm or less from the viewpoint of forming a minute abrasion trace. The length r1 may be 0.5mm to 5mm, 1mm to 3mm, or 1.5mm to 2 mm.
The angle θ between the first surface 31 and the second surface 32 of the contact 1 is 100 ° to 150 °, and the length D in the direction of the rotation axis R between the first boundary portion 31A, which is the boundary between the first surface 31 and the connection surface 33, and the second boundary portion 32A, which is the boundary between the second surface 32 and the connection surface 33, is 1 μm to 10 μm. In the present specification, as shown by the broken line in fig. 4, the angle θ formed by the first surface 31 and the second surface 32 is the angle formed by virtual planes formed by expanding the first surface 31 and the second surface 32. Thus, the wear mark formed on the single crystal diamond 75 becomes clear, and a stable wear test can be performed. This suppresses variation in the evaluation result of the micro wear characteristic, and the evaluation result is stable. In the present specification, a step of forming a wear trace on the single crystal diamond 75 using the contact 1, which is performed for evaluation of the minute wear characteristics of the single crystal diamond 75, is also referred to as a wear test.
The lower limit of the angle θ may be 100 ° or more or 110 ° or more from the viewpoint of maintaining the shape of the outer end portion 3A at the time of the wear test. The upper limit of the angle θ may be 150 ° or less or 140 ° or less from the viewpoint of forming a clear abrasion trace. The angle θ may be 100 ° or more and 150 ° or less, or 110 ° or more and 140 ° or less.
The lower limit of the length D may be 1 μm or more or 2 μm or more from the viewpoint of maintaining the shape of the contact outer end portion 3A at the time of the wear test. The upper limit of the length D may be 10 μm or less or 8 μm or less from the viewpoint of forming a clear abrasion trace. The length D may be 1 μm or more and 10 μm or less, or 2 μm or more and 8 μm or less.
As shown in fig. 4, the intersection line of the connection surface 33 and the cross section including the rotation axis R may be a straight line. This enables stable wear tests. This suppresses variation in the evaluation result of the micro wear characteristic, and the evaluation result is stable.
As shown in fig. 5, the length from the rotation axis R to the outer end portion 3A may be longer than the length from the rotation axis R to the first boundary portion 31A and longer than the length from the rotation axis R to the second boundary portion 32A. This enables stable wear tests. This suppresses variation in the evaluation result of the micro wear characteristic, and the evaluation result is stable. In the cross section including the rotation axis R, when the connection surface 33 is an arc, the radius of the arc may be 1 μm or more and 10 μm or less, or may be 2 μm or more and 8 μm or less.
As shown in fig. 1 to 3, the first portion 2 of the contact 1 preferably includes a hole formed in a portion corresponding to the rotation axis R. Thus, in the wear test, the spindle can be inserted into the hole. The contact 1 can further include a shaft fixed to the first portion 2.
An example of a method for manufacturing a contact according to the present embodiment will be described. First, high purity graphite (purity of 99.9% or more) is used as a starting material, and sintered by a direct conversion method under an ultra-high pressure to synthesize polycrystalline diamond. The sintering conditions can be, for example, temperatures of 2200 to 2300℃and pressures of 15 to 16GPa, and sintering times of 10 to 30 minutes. The polycrystalline diamond obtained was shaped into the shape of the contact according to the present embodiment by laser processing, grinding with a diamond wheel, and polishing, to obtain the contact.
Embodiment 2: method for evaluating wear characteristics in micro-regions of Single Crystal Diamond
A method for evaluating wear characteristics in a micro region of single crystal diamond 75 according to this embodiment will be described with reference to fig. 6. Fig. 6 is an overview of the wear test device used in the method for evaluating the minute wear characteristics of the present embodiment. The wear test device includes a machining center 60 and a sample holder 70. The machining center 60 includes a spindle 61 and a fixing screw 62 for fixing the contact 1 to the spindle 61. The sample holding portion 70 includes a jig 76 for holding the single crystal diamond 75, an air cylinder 71 for moving the jig 76 in the direction of the contact 1, and a linear guide 72 disposed around the air cylinder 71.
The method for evaluating wear characteristics in a micro region of a single crystal diamond according to the present embodiment includes:
A first step of pressing the single crystal diamond 75 toward the outer end 3A while rotating the contact 1 described in embodiment 1, thereby forming a wear trace on the single crystal diamond 75; and
And a second step in which the wear characteristics in the micro-regions of the single crystal diamond 75 are evaluated based on the length of the wear mark.
< First step >)
The spindle 61 of the machining center 60 is inserted into the hole of the contact 1 and fixed by the fixing screw 62. Since the contact 1 is fixed to the main shaft 61, when the main shaft 61 is rotated, the contact 1 rotates in synchronization with the main shaft 61. From the viewpoint of suppression of thermal reactive wear, the rotation speed is preferably 100rpm to 1000rpm, and/or the peripheral speed is preferably 1m/min to 10 m/min. In fig. 6, the contact 1 is fixed to the main shaft 61 by the fixing screw 62, but the method of fixing the contact 1 to the main shaft 61 is not limited thereto. For example, an adhesive can be used to fix the contact 1 and the spindle 61.
A jig 76 for fixing the single crystal diamond 75 to the sample holding portion 70. An air cylinder 71 is provided in a direction opposite to the direction of single crystal diamond 75 to which jig 76 is fixed. As shown by the arrow a in fig. 6, a constant pressure gas is fed into the cylinder 71, and a load is applied to the cylinder 71 in the arrow b direction, whereby the cylinder 71 moves in the direction of the contact 1. Thereby, the single crystal diamond 75 is pressed against the outer end portion 3A of the contact 1, and a wear trace is formed on the single crystal diamond 75. The pressing pressure is preferably 0.1MPa or more and 0.2MPa or less. The pressing time is preferably 60 seconds.
Single crystal diamond 75 has a planar surface 77, and the first step may also include: step 1-1, in which single crystal diamond 75 is arranged with plane 77 opposite to contact 1 and parallel to rotation axis R in step 1-1; and a1 st-2 nd step of pressing the single crystal diamond 75 toward the outer end 3A of the contact 1 by applying a load in the normal direction of the plane 77 to the single crystal diamond 75 in the 1 st-2 nd step. This improves the accuracy of the micro wear test. In processing to provide single crystal diamond 75 with flat surface 77, the (100) surface of single crystal diamond 75 is preferably parallel ground with a metal bond diamond grinding wheel or disc.
Plane 77 of single crystal diamond 75 is a (001) plane, and the abrasion trace may be parallel to the < 100 > direction of the (001) plane. This improves the accuracy of the micro wear test.
When a plurality of wear marks are formed on one single crystal diamond 75, the plurality of wear marks are substantially parallel, and the interval between the wear marks may be 0.05mm or more and 0.1mm or less.
Before the start of the formation of the abrasion trace, the first surface 31 and the second surface 32 of the contact 1 were directly connected to each other to form a V-shape, and when the connection surface 33 was not present, pretreatment was performed five or more times with respect to the < 100 > direction of the (001) surface of the single crystal diamond under the above-described abrasion trace formation conditions (rotation speed, pressing pressure, pressing time) before the formation of the abrasion trace for evaluation, and the length D of the outer end portion 3A was adjusted to be 1 μm or more and 10 μm or less.
< Second step >)
In the second step, the wear characteristics of single crystal diamond 75 are evaluated based on the length of the wear trace formed on single crystal diamond 75 in the first step. The wear characteristics can be evaluated by the amount of wear (removal amount), the area of the wear trace, or the length of the wear trace. In the present embodiment, the abrasion trace length is evaluated as a length that can be easily measured. The length of the wear mark was measured by an optical microscope at 500 times the observation magnification.
The method for evaluating the micro wear characteristics according to the present embodiment can evaluate the wear characteristics (wear resistance) of the micro regions of the single crystal diamond 75 with high accuracy. This allows a detailed investigation of the distribution state of wear characteristics of single crystal diamond 75 due to uneven distribution of impurities and crystal defects. This evaluation method is useful for selecting and evaluating the quality of single crystal diamond 75 when single crystal diamond 75 is used for precision cutting tools such as precision turning tools and small-diameter end mills.
Examples
The present embodiment will be described in further detail with reference to examples. However, the present embodiment is not limited to these examples.
As the test body, high-purity, colorless and transparent synthetic single crystal diamond (type IIa, impurity of 0.1ppm or less) containing almost no impurity or crystal defect and synthetic single crystal diamond (type Ib, nitrogen containing about hundred ppm as an isolated substitutional impurity) which is generally produced as industrial yellow were used. The (100) surface of each test piece was parallel-polished by a metal bond diamond grinding wheel or a grinding plate to form a flat surface, and the micro-wear characteristics were evaluated on the flat surface.
It is presumed that impurities and crystal defects affect the wear characteristics of single crystal diamond. Thus, first, in a test body composed of synthetic single crystal diamond (hereinafter, also referred to as "synthetic type IIa single crystal diamond") containing almost no impurity or crystal defect, confirmation of the validity of the present evaluation method, the loss state of the contact, and the stability (examples 1 and 2 described later) were examined.
Further, differences in orientation based on the minute wear characteristics of the synthesized type IIa single crystal diamond were evaluated (example 3 described below).
Next, a relationship between a growth sector and a micro wear characteristic was examined in a test body made of synthetic single crystal diamond (hereinafter, "synthetic type Ib single crystal diamond") produced as a general industrial use (example 4 described below).
In all of the following examples, the contact is made of polycrystalline diamond composed of a plurality of diamond particles. The plurality of diamond particles had an average particle diameter of 50nm. The knoop hardness of the polycrystalline diamond was 130GPa.
In all of the following examples, the conditions for forming the wear marks were: the rotational speed of the contact was 313rpm (peripheral speed 3.15 m/min), the pressing pressure per abrasion trace was 0.1MPa, and the pressing time was 60 seconds. The interval between abrasion marks on the test body was 0.1mm or 0.05mm.
Example 1: evaluation of micro wear characteristics in the < 100 > direction of the (001) face of the synthesized type IIa single crystal diamond
As the contact, the contact described in embodiment 1 was prepared. The contact had a V-shaped outer end (i.e., the first surface 31 and the second surface 32 intersect to form an angle θ, and the connecting surface 33 is not present), a cross-sectional shape shown in fig. 3, and a length r1 of 1.6mm (diameter in plan viewZhou Changyao 10mm of the second portion), the angle θ is 120 °, and the maximum length (thickness) of the rotation axis R direction is 0.6mm.
As shown in FIG. 7 and FIG. 8, abrasion marks were formed in parallel with the < 100 > direction of the (001) plane in the synthesized type IIa single crystal diamond. The result is shown as a solid line in the graph of fig. 10. In the coordinate system of fig. 10, the horizontal axis represents the test number, and the vertical axis represents the length (μm) of the abrasion trace. The test numbers correspond to the number of wear marks formed. For example, test number 5 refers to the formation of the fifth wear mark.
As shown in fig. 10, the length of the abrasion trace gradually becomes shorter until the fifth abrasion trace shown in test No.5 is formed. This is presumed to be because: since the second portion of the contact before the abrasion test is V-shaped and sharp, abrasion marks are easily formed, and the front end of the second portion is abraded with the increase of the number of pretreatment tests, and the abrasion marks are difficult to form. After the fifth abrasion trace is formed, the outer end portion is flattened, and the length D of the outer end portion is about 5 to 6 μm. In the formation of the wear marks after the fifth time, the outer end portions are hardly worn and stabilized, and therefore the length and width of the wear marks are almost constant. This is presumably because the abrasion resistance of polycrystalline diamond is far superior to that of single crystal diamond in the < 100 > direction of the (001) plane.
From the above, it was confirmed that stable fine wear evaluation was possible after the formation of wear marks as pretreatment was performed five or more times. In addition, it was confirmed that a stable abrasion test was performed on a test body made of single crystal diamond.
Example 2: evaluation of the micro wear characteristics of the (001) face of the synthesized IIa Single Crystal Diamond in the < 110 > direction ]
Thereafter, as shown in fig. 7 and 9, abrasion marks were formed in parallel with the < 110 > direction of the (001) plane for the synthesized type IIa single crystal diamond using the same contact as in example 1, and evaluation was performed. The result is shown as a broken line of the graph of fig. 10.
As shown in fig. 10, as the test number (the number of times of forming the abrasion trace) increases, the abrasion trace becomes shorter. This is presumably because the wear resistance of polycrystalline diamond is equal to the wear resistance in the < 110 > direction of the (001) plane of single-crystal diamond, and therefore the outer end portion of the contact continues to wear off little by little.
The following was confirmed by example 1 and example 2: for the purpose of examining the difference in abrasion resistance between crystals and the distribution state of abrasion characteristics in crystals, it is preferable to evaluate the abrasion resistance by forming abrasion marks parallel to the < 100 > direction of the (001) plane of the single crystal diamond.
Example 3: comparison of abrasion Properties of the (001) face of the synthesized IIa Single Crystal Diamond in the < 100 > and < 110 > directions
In example 1, the asymptotic value of the < 100 > direction abrasion trace length (hereinafter, also referred to as "< 100 > abrasion trace length") of the (001) face of the synthesized IIa single crystal diamond was about 145 to 150 μm. On the other hand, in example 2, the abrasion trace length in the < 110 > direction (hereinafter, also referred to as "< 110 > abrasion trace length") of the (001) face of the synthesized IIa single crystal diamond at the start of the test (test No. 1) was about 110 to 120 μm. Therefore, the abrasion trace length of < 100 > is about 1.3 times the abrasion trace length of < 110 > and about 2.2 times the abrasion volume.
The above results are the same as experimental results and trends of the metal bond diamond grinding wheel based on non-patent document 2, but in the contact according to the present embodiment, since the abrasion (collapse) of the outer end portion is very small, the difference between the difference by crystal and the difference by position in the crystal can be evaluated more accurately.
From examples 1 to 3, it was confirmed that: according to the evaluation method using the contact according to the present embodiment, the difference due to the surface orientation of the wear characteristics (characteristics related to the inherent wear resistance of diamond) of single crystal diamond can be accurately evaluated even in a micro region of the order of several tens μm.
Example 4: evaluation of relationship between growth sector and micro wear characteristics of synthetic Ib Single Crystal Diamond
As the contact, the contact described in embodiment 1 was prepared. The contact had a cross-sectional shape shown in FIG. 3, and a length r1 of 1.6mm (diameter in plan viewZhou Changyao 10mm of the second portion), the angle θ being 120 °, the length D being 5 μm, the maximum length (thickness) in the direction of the axis of rotation R being 0.6mm.
The relationship between the growth sector and the micro wear characteristics was evaluated by forming wear marks parallel to the < 100 > direction of the (001) plane on a test body of the synthesized type Ib single crystal diamond containing about 100ppm of nitrogen impurities using the above-mentioned contact. Two of the above test bodies were prepared. Hereinafter, they will be referred to as "test body a" and "test body B", respectively.
The distribution of the growth sectors in the test piece a and the test piece B was confirmed by observation of ultraviolet excitation fluorescent images. FIG. 11 is a photograph substitute drawing showing an ultraviolet excited fluorescent image of the specimen A. FIG. 13 is a photograph substitute drawing showing an ultraviolet excited fluorescent image of the specimen B. In fig. 13, the abrasion trace observed by the optical microscope is superimposed on the ultraviolet excited fluorescent image.
Fig. 12 is a graph showing the relationship between the test number and the wear mark length in the test body a. In fig. 12, test numbers 7 to 12 represent wear marks formed in the (111) sector, test numbers 13 to 27 represent wear marks formed in the (100) sector, and test number 28 represents wear marks formed in the (110) sector.
Fig. 14 is a graph showing the relationship between the test number and the wear mark length in the test body B. In fig. 14, test No. 5 shows wear marks formed in the (110) sector, test nos. 6 to 26 show wear marks formed in the (100) sector, and test No. 27 shows wear marks formed in the (110) sector.
From fig. 12 and 14, it was confirmed that the wear characteristics were different depending on the growth sector, and particularly the wear resistance of the (110) sector was very high. The nitrogen amount in each of the grown sectors is generally known as (111) > (100) > (113) > (110), and the nitrogen is hardly contained in the (110) sector. Therefore, the abrasion loss of the sector portion is presumed to be small (110).
From the above, it was confirmed by the method of evaluating the micro wear characteristics of single crystal diamond using the contact according to the present embodiment that the wear resistance of single crystal diamond containing impurities varies depending on the growth sector and that the distribution state of impurities is greatly affected.
As described above, the embodiments and examples of the present disclosure have been described, but it is originally intended that the configurations of the embodiments and examples be appropriately combined and variously modified.
The presently disclosed embodiments and examples are considered in all respects as illustrative and not restrictive. The scope of the present invention is defined by the claims and is not limited to the embodiments and examples described above, but is intended to include all modifications within the meaning and scope equivalent to the claims.
Reference numerals illustrate:
1: a contact;
2: a first portion;
3: a second portion;
3A: an outer end portion;
31: a first face;
32: a second face;
31A: a first boundary portion;
32A: a second boundary portion;
33: a connection surface;
R: a rotation shaft;
60: a machining center;
61: a main shaft;
62: a fixing screw;
70: a sample holding section;
71: a cylinder;
72: a linear guide;
75: single crystal diamond;
76: a clamp;
77: a plane.
Claims (7)
1. A contact is an annular contact made of polycrystalline diamond composed of a plurality of diamond particles, wherein,
The contact is configured such that the rotation shaft passes through the center,
The contact is provided with:
a first portion having a constant thickness in a radial direction and including an inner end portion; and
A second portion having a radially reduced thickness and comprising an outer end portion,
The second portion has:
A first face continuous with an upper surface of the first portion; a second surface continuous with a lower surface of the first portion; and a connecting surface connecting the first surface with the second surface and including the outer end portion,
In a section along the axis of rotation,
An angle θ between a first line segment representing the first surface and a second line segment representing the second surface is 100 DEG or more and 150 DEG or less,
A length between a first boundary portion which is a boundary between the first surface and the connection surface and a second boundary portion which is a boundary between the second surface and the connection surface is 1 μm or more and 10 μm or less,
The length from the rotation shaft to the outer end is 0.5mm or more and 5mm or less,
The plurality of diamond particles have an average particle diameter of 10nm to 300 nm.
2. The contact of claim 1, wherein the polycrystalline diamond has a knoop hardness of 120GPa or greater.
3. A contact according to claim 1 or 2, wherein the intersection of the connection face with a section plane containing the rotation axis is a straight line.
4. The contact according to claim 1 or 2, wherein a length from the rotation axis to an end of the contact is greater than a length from the rotation axis to the first boundary portion and greater than a length from the rotation axis to the second boundary portion.
5. An evaluation method of wear characteristics in a micro region of a single crystal diamond,
The evaluation method includes:
A first step of forming a wear mark on the single crystal diamond by pressing the single crystal diamond toward the outer end portion while rotating the contact according to any one of claims 1 to 4; and
And a second step in which wear characteristics in a micro region of the single crystal diamond are evaluated based on the length of the wear trace.
6. The evaluation method according to claim 5, wherein,
The single crystal diamond has a planar surface and,
The first step comprises:
A step 1-1 in which the single crystal diamond is arranged such that the plane faces the contact and is parallel to the rotation axis in the step 1-1; and
And 1-2 steps of pressing the single crystal diamond toward the outer end portion by applying a load in a direction normal to the plane to the single crystal diamond in the 1-2 steps.
7. The evaluation method according to claim 6, wherein,
The plane of the single crystal diamond is the (001) plane,
The wear trace is parallel to the < 100 > direction of the (001) face.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2021183404 | 2021-11-10 | ||
| JP2021-183404 | 2021-11-10 | ||
| PCT/JP2022/038211 WO2023084988A1 (en) | 2021-11-10 | 2022-10-13 | Contact, and method for evaluating microwear properties of single-crystal diamond using same |
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| CN118103688A true CN118103688A (en) | 2024-05-28 |
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| CN202280069324.3A Pending CN118103688A (en) | 2021-11-10 | 2022-10-13 | Contact and method for evaluating micro-wear characteristics of single crystal diamond using same |
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| EP (1) | EP4431906A1 (en) |
| JP (1) | JP7556479B2 (en) |
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| US8434347B2 (en) | 2009-12-18 | 2013-05-07 | Varel Europe S.A.S. | Synthetic materials for PDC cutter testing or for testing other superhard materials |
| JP6007732B2 (en) | 2012-11-06 | 2016-10-12 | 住友電気工業株式会社 | Polycrystalline diamond and method for producing the same |
| CN105158098B (en) | 2015-08-26 | 2017-10-31 | 南京航空航天大学 | A kind of controllable single grain grinding test platform of abrasive particle pose and its test method |
| JP2019066366A (en) | 2017-10-03 | 2019-04-25 | 英二 草野 | Sample holding stand |
| JP2021183404A (en) | 2020-05-22 | 2021-12-02 | キヤノン株式会社 | Substrate for liquid discharge head and method for manufacturing the same |
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- 2022-10-13 JP JP2023559497A patent/JP7556479B2/en active Active
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